CN105016389A - Carbon shell-coated lead molybdate nanocrystal and preparation method thereof - Google Patents
Carbon shell-coated lead molybdate nanocrystal and preparation method thereof Download PDFInfo
- Publication number
- CN105016389A CN105016389A CN201510412852.6A CN201510412852A CN105016389A CN 105016389 A CN105016389 A CN 105016389A CN 201510412852 A CN201510412852 A CN 201510412852A CN 105016389 A CN105016389 A CN 105016389A
- Authority
- CN
- China
- Prior art keywords
- nanocrystal
- coated
- lead molybdate
- preparation
- reactor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a carbon shell-coated lead molybdate nanocrystal and its preparation method. Citric acid is used to control synthesis of lead molybdate nanometer materials with different carbon shell thicknesses. Specifically, the preparation method is simple and novel and has strong controllability. The synthesized carbon layer-coated lead molybdate composite nanocrystal has high purity, and length and width of the nanocrystal are about 100 nm and 50 nm. In addition, the carbon shell coated outside the obtained lead molybdate composite material is more beneficial to separation and transfer of electrons. The carbon shell-coated lead molybdate nanocrystal is used as a cathode material for photoelectrocatalytic water-splitting, and stability and catalytic efficiency of the material also can be enhanced. The invention accords with researches on the latest clean energy and sustainable energy sources.
Description
Technical field
The present invention relates to materials synthesis field, relate to the application of semiconductor nano material in hydrogen energy source field that the coated semiconductor nano material of a kind of carbon shell and synthetic method and described carbon shell thereof are coated particularly, more particularly relate to use citric acid to control to synthesize the lead molybdate nano material of different carbon thickness of the shell, relate to prepared lead molybdate and the coated application of lead molybdate nano material in photoelectrocatalysis splitting water of carbon thereof in addition.
Background technology
Hydrogen is a kind of clean, free of contamination novel energy, is expected to substitute fossil fuels, meets global energy requirements, alleviating energy crisis.At present, utilize sunlight to carry out photoelectrocatalysis splitting water and prepare hydrogen there is environmental protection and energy saving, the advantage such as sustainable, become the focus that people pay close attention to.But the semi-conducting electrode material in present stage light photoelectrocatalysis splitting water device is still subject to serious restriction, cause that the efficiency of photoelectrocatalysis cracking aquatic products hydrogen is low, industrialization cost is high and the problem such as poor stability.
Lead molybdate is as the important p-type semiconductor material of a class, and its band-gap energy is 3.2eV, and wherein Valence-band is about-0.6eV, and conduction band energy is about 2.6eV, is conventional photoluminescence, scintillator, sensor and photocatalyst material.In addition, relative to other common semiconductor material, lead molybdate exists with sheelite form at occurring in nature, and rich reserves, use cost is low.But p-type semiconductor exists a serious defect as the cathode material of photoelectrochemistry water of decomposition, work long hours exactly and easily reduced by electrolytic solution, stability is poor, and the life-span is shorter.Therefore, University of Texas-Austin of the U.S. has synthesized the p-PbMoO of p-n junction
4/ n-Bi
2o
3nano composite material, and test the performance (J.Phys.Chem.Lett.2013,4,2707-2710) of this material at photoelectrocatalysis splitting water.Test data shows: the stability of the p-n junction nano composite material of formation improves.But the compound of this semi-conductor and semi-conductor, reduces the electroconductibility of material, have impact on its photocatalysis efficiency; And in preparation process, there is the problems such as complex process, cost be higher.
Summary of the invention
In the present invention, contriver uses citric acid to carry out controlled synthesis lead molybdate and the coated lead molybdate of carbon is nanocrystalline in solvent process for thermosynthesizing.It is the coated lead molybdate nanocrystals of 2 to 20 nanometers that the citric acid adding different amount in reaction soln can obtain carbon thickness of the shell.Find by measuring, the carbon-coating outside lead molybdate can promote the electroconductibility of material, stops lead molybdate to be corroded by electrolyte solution.Therefore the lead molybdate nanocrystal that prepared carbon shell is coated is nanocrystalline relative to exposed lead molybdate, and the efficiency of its photoelectrocatalysis splitting water and stability obtain larger lifting.
One object of the present invention is the lead molybdate nanocrystal providing a kind of carbon shell coated, and the carbon thickness of the shell of described lead molybdate nanocrystal is 2 to 20 nanometers, is preferably 2 to 10 nanometers, is more preferably 2 to 8 nanometers.Can be such as 2 nanometers, 5 nanometers or 8 nanometers, most preferably be 2 nanometers, its length and width be about 50 to 100 nanometers and 20 to 50 ran.
Another object of the present invention is the preparation method of the lead molybdate nanocrystal providing a kind of carbon shell coated, and described preparation method comprises:
1) at room temperature, be plumbous and seven Ammonium paramolybdate tetrahydrates of three acetate hydrate of 1:1 by mol ratio, and appropriate solvent add reactor polytetrafluoroethyllining lining in and stir 2 to 15 minutes;
2) and seven Ammonium paramolybdate tetrahydrates plumbous based on three acetate hydrate of 100 weight parts altogether, join aforesaid reaction vessel inside liner by the citric acid of 100-2000 weight part, then continue stirring 5 to 10 minutes;
3) reactor is put in the electric drying oven with forced convection of 100-240 degree after tightening kettle cover, and keep 30-90 minute;
4) take out reactor and naturally cool to room temperature state, subsequently, repeatedly intersect centrifugal, washed product with dehydrated alcohol and deionized water, and in vacuum drying oven desciccate.Thus obtain the product of white.
Preferably, step 1 in the preparation method of the coated lead molybdate nanocrystal of carbon shell according to the present invention) in one or more in solvent selected from methanol, ethanol and deionized water, be more preferably deionized water, plumbous and seven Ammonium paramolybdate tetrahydrates of three acetate hydrate based on 100 weight parts altogether, the amount of described solvent is 5-20 weight part.
Preferably, step 2 in the preparation method of the coated lead molybdate nanocrystal of carbon shell according to the present invention) in, plumbous and seven Ammonium paramolybdate tetrahydrates of three acetate hydrate based on 100 weight parts altogether, the add-on of citric acid is 100-1200 weight part, be preferably 100-1050 weight part, be more preferably 105-1050 weight part, most preferably be and be selected from 105 weight parts, 210 weight parts or 1050 weight parts.
Beneficial effect
The present invention has following advantage: this type of synthetic method is simple, novel, controllability is strong.Utilize citric acid pyrolytic decomposition to prepare the carbon nanometer layer of different thickness, cost be low, environmental protection, pollution-free.The coated lead molybdate composite nanocrystal purity of carbon material of synthesis is high, length and width thereof are about 100 nanometers and 50 ran.In addition, carbon shell coated outside the lead molybdate matrix material of acquisition, is more conducive to separation and the transfer of electronics.As the cathode material of photoelectrochemistry water of decomposition, its stability and catalytic efficiency can also be improved, and also meet the research of up-to-date clean energy and sustainable energy aspect thereof.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of embodiment product, wherein photo 1 is the lead molybdate nanocrystal coated according to 2 nano-sized carbon shells of embodiment 1 preparation, photo 2 is the lead molybdate nanocrystal coated according to 5 nano-sized carbon shells of embodiment 2 preparation, photo 3 is the lead molybdate nanocrystal coated according to 8 nano-sized carbon shells of embodiment 3 preparation, and photo 4 is the lead molybdate nanocrystal of the non-carbon coated shell according to embodiment 4 preparation;
Fig. 2 is the X-ray powder diffraction figure of sample obtained according to embodiment, the lead molybdate nanocrystal that the coated lead molybdate nanocrystal of the lead molybdate nanocrystal that in figure, curve 1,2,3,4 represents the non-carbon coated shell prepared according to embodiment 4 respectively, the 2 nano-sized carbon shells prepared according to embodiment 1, the 5 nano-sized carbon shells prepared according to embodiment 2 are coated and the coated lead molybdate of the 8 nano-sized carbon shells prepared according to embodiment 3 nanocrystalline;
Fig. 3 is the high-resolution electron microscope photo of sample obtained according to embodiment, the lead molybdate nanocrystal that the coated lead molybdate nanocrystal of the lead molybdate nanocrystal that in figure, photo 1,2,3,4 represents the non-carbon coated shell prepared according to embodiment 4 respectively, the 2 nano-sized carbon shells prepared according to embodiment 1, the 5 nano-sized carbon shells prepared according to embodiment 2 are coated and the coated lead molybdate of the 8 nano-sized carbon shells prepared according to embodiment 3 nanocrystalline;
Fig. 4 is the Raman spectrogram of the sample according to embodiment acquisition, the lead molybdate that in figure, curve 1,2,3,4 represents the coated lead molybdate nanocrystal of the lead molybdate nanocrystal of the non-carbon coated shell prepared according to embodiment 4, the coated lead molybdate nanocrystal of 2 nano-sized carbon shells prepared according to embodiment 1, the 5 nano-sized carbon shells prepared according to embodiment 2 respectively and the 8 nano-sized carbon shells prepared according to embodiment 3 are coated is nanocrystalline, wherein I, II represent D band respectively and are with G, and its position is approximately 1363cm
-1with 1595cm
-1.Simultaneously D band and G are with what represent respectively to be the carbon of lack of alignment and orderly graphite carbon, and it is carbon shell that this Raman spectrogram describes Lead molybdate nano crystal material surface coated;
Fig. 5 is the linear sweep voltammetry graphic representation of sample when photoelectrochemistry water-splitting obtained according to embodiment, and in figure, curve 1 represents the blank FTO (SnO of doped with fluorine of non-coated samples
2transparent conducting glass), curve 2,3,4,5 represents the lead molybdate nanocrystal of the non-carbon coated shell according to embodiment 4 preparation be coated on blank FTO, lead molybdate nanocrystal, according to 5 nano-sized carbon shells of the embodiment 2 preparation coated lead molybdate nanocrystal that be coated in blank FTO on coated according to 2 nano-sized carbon shells of embodiment 1 preparation be coated on blank FTO respectively, is coated in the lead molybdate nanocrystal coated according to 8 nano-sized carbon shells of embodiment 3 preparation on blank FTO.
Embodiment
Following examples are only enumerate as the example of embodiment of the present invention, do not form any restriction to the present invention, it will be appreciated by those skilled in the art that the amendment in the scope not departing from essence of the present invention and design all falls into protection scope of the present invention.
The instrument used in an embodiment has:
(model is x-ray powder diffraction instrument: Rigaku D/Max 2200PC, wherein copper K
αradiation diffraction instrument (
) and graphite monochromator scanning angle from 10 °-80 ° and sweep velocity per minute 5.0 °); Transmission electron microscope (model is: JEM100-CXII); High-resolution-ration transmission electric-lens (model is: GEOL-2010); Raman spectrometer (model is: NEXUS 670), electrochemical workstation (model is: CHI 660D), (it comprises photoelectrochemistry water-splitting tester: 350 watts of xenon lamps, the spectral filter of different wave length, camera bellows, LP-3A laser power meter) (Beijing Heng Gong Instrument Ltd.).
The chemical reagent three acetate hydrate lead used and ammonium molybdate are commercially available reagent pure reagent.
The synthesis of the lead molybdate nanocrystal that embodiment 1:2 nano-sized carbon shell is coated
First three acetate hydrate lead (75.9 milligrams) and ammonium molybdate (35.3 milligrams) at room temperature being joined a volume is in the polytetrafluoroethyllining lining of 20 milliliters, with liquid-transfering gun, the deionized water of 12.0 milliliters is joined in polytetrafluoroethyllining lining subsequently, the solution of above-mentioned acquisition is placed on magnetic stirring apparatus and stirs 10 minutes.
The citric acid of 105.0 milligrams is joined in above-mentioned liquid, then the solution obtained in above-mentioned reaction liner is stirred 5 minutes on magnetic stirring apparatus.
Next, the reaction liner that precursor aqueous solution is housed is put into the reactor of stainless steel casing, tighten kettle cover, then reactor is put in the electric drying oven with forced convection of 200 degree, and keep 1 hour.
After reaction terminates, by the reactor cool to room temperature state of taking out, the solution in reaction liner is transferred in the centrifuge tube of 10ml, by the solution dehydrated alcohol in centrifuge tube and deionization waterside cross washing 3 times, centrifugally just obtain white precipitate; The white precipitate obtained is placed on drying in the vacuum drying oven of 50 degree and just obtains final product.
The transmission electron microscope photo of the finished product that the photo 1 of Fig. 1 is prepared for the present embodiment, its length and the width of this photo display preparation are about 50 to 100 nanometers and 20 to 50 ran; The X-ray powder diffraction figure of the finished product that the curve 2 in Fig. 2 is prepared for the present embodiment, as can be seen from the figure, it is high to synthesize the product degree of crystallinity obtained under hydrothermal conditions; The high-resolution electron microscope photo of the finished product that the photo 2 in Fig. 3 is prepared for the present embodiment; The Raman spectrogram of the finished product that the curve 2 of Fig. 4 is prepared for the present embodiment, in this Raman spectrum, have absorption band D to be be with G, its position is approximately 1363cm
-1with 1595cm
-1, illustrate lead molybdate nanocrystal outside surface prepared by the present embodiment coated be carbon shell.
The lead molybdate nanocrystal that embodiment 2:5 nano-sized carbon shell is coated
Except the citric acid adding 210.0 milligrams, prepare the coated lead molybdate nanocrystal of 5 nano-sized carbon shells according to the method that embodiment 1 is identical.
The transmission electron microscope photo of the finished product that the photo 2 of Fig. 1 is prepared for the present embodiment, its length and the width of this photo display preparation are about 50 to 100 nanometers and 20 to 50 ran; The X-ray powder diffraction figure of the finished product that the curve 3 in Fig. 2 is prepared for the present embodiment, as can be seen from the figure, it is high to synthesize the product degree of crystallinity obtained under hydrothermal conditions; The high-resolution electron microscope photo of the finished product that the photo 3 in Fig. 3 is prepared for the present embodiment; The Raman spectrogram of the finished product that the curve 3 of Fig. 4 is prepared for the present embodiment, in this Raman spectrum, have absorption band D to be be with G, its position is approximately 1363cm
-1with 1595cm
-1, illustrate lead molybdate nanocrystal outside surface prepared by the present embodiment coated be carbon shell.
The lead molybdate nanocrystal that embodiment 3:8 nano-sized carbon shell is coated
Except the citric acid adding 1050 milligrams, prepare the coated lead molybdate nanocrystal of 8 nano-sized carbon shells according to the method that embodiment 1 is identical.
The transmission electron microscope photo of the finished product that the photo 3 of Fig. 1 is prepared for the present embodiment, its length and the width of this photo display preparation are about 50 to 100 nanometers and 20 to 50 ran; The X-ray powder diffraction figure of the finished product that the curve 4 in Fig. 2 is prepared for the present embodiment, as can be seen from the figure, it is high to synthesize the product degree of crystallinity obtained under hydrothermal conditions; The high-resolution electron microscope photo of the finished product that the photo 4 in Fig. 3 is prepared for the present embodiment; The Raman spectrogram of the finished product that the curve 4 of Fig. 4 is prepared for the present embodiment, in this Raman spectrum, have absorption band D to be be with G, its position is approximately 1363cm
-1with 1595cm
-1, illustrate lead molybdate nanocrystal outside surface prepared by the present embodiment coated be carbon shell.
Embodiment 4: the lead molybdate nanocrystal of non-carbon coated shell
Except not adding except citric acid, prepare the lead molybdate nanocrystal of non-carbon coated shell according to the method that embodiment 1 is identical.
The transmission electron microscope photo of the finished product that the photo 1 of Fig. 1 is prepared for the present embodiment, its length and the width of this photo display preparation are about 50 to 100 nanometers and 20 to 50 ran; The X-ray powder diffraction figure of the finished product that the curve 1 in Fig. 2 is prepared for the present embodiment, as can be seen from the figure, it is high to synthesize the product degree of crystallinity obtained under hydrothermal conditions; The high-resolution electron microscope photo of the finished product that the photo 1 in Fig. 3 is prepared for the present embodiment; The Raman spectrogram of the finished product that the curve 1 of Fig. 4 is prepared for the present embodiment, in this Raman spectrum, have absorption band D to be be with G, its position is approximately 1363cm
-1with 1595cm
-1, illustrate lead molybdate nanocrystal outside surface prepared by the present embodiment coated be carbon shell.
Test example: photoelectrochemistry water-splitting is tested
Adopt the sample of preparation and the SnO of blank doped with fluorine in photoelectrocatalysis splitting water tester testing example 1 to 4
2the performance of the photoelectrochemistry water-splitting of transparent conducting glass (FTO).
First, respectively the sample of preparation in embodiment 1 to 4 is dispersed in hexanaphthene respectively, is then dropwise coated with and is added to above clean blank FTO, drying 1 hour under the nitrogen atmosphere of 60 degree afterwards.Then, the sample the first step obtained is put into respectively in the electrolyzer of the 100 ml water solution containing 0.5 mol sulfuric acid and tests, and different samples obtains different density of photocurrent numerical value.Test result shows: the lead molybdate nanocrystal coated compared to the carbon-free shell of preparation in embodiment 4, the lead molybdate nanocrystal having different thickness carbon shell coated has good performance in photoelectrochemistry water-splitting, meanwhile, coated outside lead molybdate carbon material is more conducive to the separation of electronics and transfer and also improves material water splitting stability of solution.
Fig. 5 is the linear sweep voltammetry graphic representation of sample when photoelectrochemistry water-splitting obtained according to embodiment, in figure, curve 1 represents the blank FTO (the SnO2 transparent conducting glass of doped with fluorine) of non-coated samples, curve 2, 3, 4, 5 respectively representative be coated in the lead molybdate nanocrystal of non-carbon coated shell prepared according to embodiment 4 on blank FTO, be coated in the lead molybdate nanocrystal coated according to 2 nano-sized carbon shells of embodiment 1 preparation on blank FTO, be coated in the lead molybdate nanocrystal coated according to 5 nano-sized carbon shells of embodiment 2 preparation on blank FTO, the lead molybdate nanocrystal coated according to 8 nano-sized carbon shells of embodiment 3 preparation be coated on blank FTO can obtain from Fig. 5: compared to standard hydrogen electrode, the lead molybdate nanocrystal that the 2 nano-sized carbon shells that embodiment 1 obtains are coated, the lead molybdate nanocrystal that the 5 nano-sized carbon shells that embodiment 2 obtains are coated, the lead molybdate nanocrystal that the 8 nano-sized carbon shells that embodiment 3 obtains are coated, the density of photocurrent of the lead molybdate nanocrystal that the non-carbon shell that embodiment 4 obtains is coated is respectively 2.7, 1.8, 1.6, 0.5 (milliampere/square centimeter).Meanwhile, further comparative result shows: in the sample that the ownership system is standby, and the coated lead molybdate nanocrystal of the 2 nano-sized carbon shells that embodiment 1 obtains is best in photoelectrocatalysis cracking aquatic products hydrogen and stability thereof.
Claims (8)
1. the lead molybdate nanocrystal that a carbon shell is coated, the carbon thickness of the shell of described lead molybdate nanocrystal is 2 to 20 nanometers, be preferably 2 to 10 nanometers, be more preferably 2 to 8 nanometers, the length of the lead molybdate nanocrystal that described carbon shell is coated and width are about 50 to 100 nanometers and 20 to 50 ran.
2. the lead molybdate nanocrystal that carbon shell according to claim 1 is coated, is characterized in that, described carbon thickness of the shell is 2 nanometers, 5 nanometers or 8 nanometers, most preferably is 2 nanometers.
3., according to a preparation method for the coated lead molybdate nanocrystal of the carbon shell of claim 1 or 2, described preparation method comprises:
1) at room temperature, be plumbous and seven Ammonium paramolybdate tetrahydrates of three acetate hydrate of 1:1 by mol ratio, and appropriate solvent add reactor polytetrafluoroethyllining lining in and stir 2 to 15 minutes;
2) and seven Ammonium paramolybdate tetrahydrates plumbous based on three acetate hydrate of 100 weight parts altogether, join aforesaid reaction vessel inside liner by the citric acid of 100-2000 weight part, then continue stirring 5 to 10 minutes;
3) reactor is put in the electric drying oven with forced convection of 100-240 degree after tightening kettle cover, and keep 30-90 minute;
4) take out reactor and naturally cool to room temperature state, subsequently, intersect centrifugal, washed product 2-5 time with dehydrated alcohol and deionized water, and in vacuum drying oven desciccate.Thus obtain the product of white.
4. the preparation method of the lead molybdate nanocrystal that carbon shell according to claim 3 is coated, it is characterized in that, step 1 in described preparation method) in one or more in solvent selected from methanol, ethanol and deionized water, be preferably deionized water, plumbous and seven Ammonium paramolybdate tetrahydrates of three acetate hydrate based on 100 weight parts altogether, the amount of described solvent is 5-20 weight part.
5. the preparation method of the lead molybdate nanocrystal that carbon shell according to claim 3 is coated, it is characterized in that, step 2 in described preparation method processed) in, plumbous and seven Ammonium paramolybdate tetrahydrates of three acetate hydrate based on 100 weight parts altogether, the add-on of citric acid is 100-1200 weight part, be preferably 100-1050 weight part, be more preferably 105-1050 weight part, most preferably be and be selected from 105 weight parts, 210 weight parts or 1050 weight parts.
6. the preparation method of the lead molybdate nanocrystal that carbon shell according to claim 3 is coated, it is characterized in that, first it is in the polytetrafluoroethyllining lining of 20 milliliters that 75.9 milligram of three acetate hydrate is plumbous and 35.3 milligrams of ammonium molybdates at room temperature join volume, with liquid-transfering gun, the deionized water of 12.0 milliliters is joined in polytetrafluoroethyllining lining subsequently, the solution of above-mentioned acquisition is placed on magnetic stirring apparatus and stirs 10 minutes, then the citric acid of 105.0 milligrams is joined in above-mentioned liquid, again the solution obtained in above-mentioned reaction liner is stirred 5 minutes on magnetic stirring apparatus, next, the reaction liner that precursor aqueous solution is housed is put into the reactor of stainless steel casing, tighten kettle cover, again reactor is put in the electric drying oven with forced convection of 200 degree, and keep 1 hour, after reaction terminates, by the reactor cool to room temperature state of taking out, solution in reaction liner is transferred in the centrifuge tube of 10ml, by the solution dehydrated alcohol in centrifuge tube and deionization waterside cross washing 3 times, centrifugally just obtain white precipitate, the white precipitate obtained is placed on drying in the vacuum drying oven of 50 degree and just obtains final product.
7. the preparation method of the lead molybdate nanocrystal that carbon shell according to claim 3 is coated, it is characterized in that, first it is in the polytetrafluoroethyllining lining of 20 milliliters that 75.9 milligram of three acetate hydrate is plumbous and 35.3 milligrams of ammonium molybdates at room temperature join volume, with liquid-transfering gun, the deionized water of 12.0 milliliters is joined in polytetrafluoroethyllining lining subsequently, the solution of above-mentioned acquisition is placed on magnetic stirring apparatus and stirs 10 minutes, then the citric acid of 210.0 milligrams is joined in above-mentioned liquid, again the solution obtained in above-mentioned reaction liner is stirred 5 minutes on magnetic stirring apparatus, next, the reaction liner that precursor aqueous solution is housed is put into the reactor of stainless steel casing, tighten kettle cover, again reactor is put in the electric drying oven with forced convection of 200 degree, and keep 1 hour, after reaction terminates, by the reactor cool to room temperature state of taking out, solution in reaction liner is transferred in the centrifuge tube of 10ml, by the solution dehydrated alcohol in centrifuge tube and deionization waterside cross washing 3 times, centrifugally just obtain white precipitate, the white precipitate obtained is placed on drying in the vacuum drying oven of 50 degree and just obtains final product.
8. the preparation method of the lead molybdate nanocrystal that carbon shell according to claim 3 is coated, it is characterized in that, first it is in the polytetrafluoroethyllining lining of 20 milliliters that 75.9 milligram of three acetate hydrate is plumbous and 35.3 milligrams of ammonium molybdates at room temperature join volume, with liquid-transfering gun, the deionized water of 12.0 milliliters is joined in polytetrafluoroethyllining lining subsequently, the solution of above-mentioned acquisition is placed on magnetic stirring apparatus and stirs 10 minutes, then the citric acid of 1050 milligrams is joined in above-mentioned liquid, again the solution obtained in above-mentioned reaction liner is stirred 5 minutes on magnetic stirring apparatus, next, the reaction liner that precursor aqueous solution is housed is put into the reactor of stainless steel casing, tighten kettle cover, again reactor is put in the electric drying oven with forced convection of 200 degree, and keep 1 hour, after reaction terminates, by the reactor cool to room temperature state of taking out, solution in reaction liner is transferred in the centrifuge tube of 10ml, by the solution dehydrated alcohol in centrifuge tube and deionization waterside cross washing 3 times, centrifugally just obtain white precipitate, the white precipitate obtained is placed on drying in the vacuum drying oven of 50 degree and just obtains final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510412852.6A CN105016389B (en) | 2015-07-14 | 2015-07-14 | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510412852.6A CN105016389B (en) | 2015-07-14 | 2015-07-14 | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105016389A true CN105016389A (en) | 2015-11-04 |
| CN105016389B CN105016389B (en) | 2016-10-19 |
Family
ID=54406769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510412852.6A Expired - Fee Related CN105016389B (en) | 2015-07-14 | 2015-07-14 | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105016389B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824086A (en) * | 2017-03-20 | 2017-06-13 | 东华理工大学 | A kind of carbosphere Quito point loads the preparation method of heterogeneous structure material |
| CN112891532A (en) * | 2021-01-27 | 2021-06-04 | 深圳技术大学 | Nano photo-thermal conversion material and preparation method and application thereof |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3567477A (en) * | 1967-11-15 | 1971-03-02 | Du Pont | Molybdate orange pigment |
| JPH01199757A (en) * | 1988-01-30 | 1989-08-11 | Tokin Corp | Grind processing method using c-grindstone and processing method for pbmoo4 monocrystal |
| JPH01305884A (en) * | 1988-06-03 | 1989-12-11 | Tokin Corp | Method of growing lead molybdate single crystal |
| WO1999052629A1 (en) * | 1998-04-15 | 1999-10-21 | Lehigh University | In-situ formation of metal-molybdate catalysts |
| RU2164562C1 (en) * | 2000-02-18 | 2001-03-27 | Аненков Александр Николаевич | Method of producing lead-tungstate scintillation single crystal |
| CN1635194A (en) * | 2003-12-30 | 2005-07-06 | 宁波大学 | Falling crucible method growth process for lead molybdate single crystal |
| CN102010006A (en) * | 2010-12-24 | 2011-04-13 | 金堆城钼业股份有限公司 | Synthesis method for lead molybdate |
| CN102071466A (en) * | 2010-12-24 | 2011-05-25 | 金堆城钼业股份有限公司 | Method for preparing lead molybdate polycrystalline material |
| CN102689922A (en) * | 2011-03-24 | 2012-09-26 | 杨春晓 | Lead compound nano-powder preparation method for recovery and manufacture of lead-acid battery |
| CN103387263A (en) * | 2013-07-11 | 2013-11-13 | 洛阳理工学院 | Lead molybdate nano crystal material and preparation method thereof |
| CN103754935A (en) * | 2014-01-07 | 2014-04-30 | 洛阳理工学院 | Method for synthesizing lead molybdate tower crystal at room temperature |
| CN103877984A (en) * | 2014-03-06 | 2014-06-25 | 同济大学 | Preparation method of Fe3O4@C@PbMoO4 core-shell magnetic nano-material |
| CN104312096A (en) * | 2013-10-11 | 2015-01-28 | 南亚塑胶工业股份有限公司 | Inorganic filler with molybdenum compound coated on surface and application thereof |
| CN105056965A (en) * | 2015-07-20 | 2015-11-18 | 长安大学 | Biological carbon sphere supported FeMoO4 Fenton catalyst, preparation method and application |
-
2015
- 2015-07-14 CN CN201510412852.6A patent/CN105016389B/en not_active Expired - Fee Related
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3567477A (en) * | 1967-11-15 | 1971-03-02 | Du Pont | Molybdate orange pigment |
| JPH01199757A (en) * | 1988-01-30 | 1989-08-11 | Tokin Corp | Grind processing method using c-grindstone and processing method for pbmoo4 monocrystal |
| JPH01305884A (en) * | 1988-06-03 | 1989-12-11 | Tokin Corp | Method of growing lead molybdate single crystal |
| WO1999052629A1 (en) * | 1998-04-15 | 1999-10-21 | Lehigh University | In-situ formation of metal-molybdate catalysts |
| RU2164562C1 (en) * | 2000-02-18 | 2001-03-27 | Аненков Александр Николаевич | Method of producing lead-tungstate scintillation single crystal |
| CN1635194A (en) * | 2003-12-30 | 2005-07-06 | 宁波大学 | Falling crucible method growth process for lead molybdate single crystal |
| CN102010006A (en) * | 2010-12-24 | 2011-04-13 | 金堆城钼业股份有限公司 | Synthesis method for lead molybdate |
| CN102071466A (en) * | 2010-12-24 | 2011-05-25 | 金堆城钼业股份有限公司 | Method for preparing lead molybdate polycrystalline material |
| CN102689922A (en) * | 2011-03-24 | 2012-09-26 | 杨春晓 | Lead compound nano-powder preparation method for recovery and manufacture of lead-acid battery |
| CN103387263A (en) * | 2013-07-11 | 2013-11-13 | 洛阳理工学院 | Lead molybdate nano crystal material and preparation method thereof |
| CN104312096A (en) * | 2013-10-11 | 2015-01-28 | 南亚塑胶工业股份有限公司 | Inorganic filler with molybdenum compound coated on surface and application thereof |
| CN103754935A (en) * | 2014-01-07 | 2014-04-30 | 洛阳理工学院 | Method for synthesizing lead molybdate tower crystal at room temperature |
| CN103877984A (en) * | 2014-03-06 | 2014-06-25 | 同济大学 | Preparation method of Fe3O4@C@PbMoO4 core-shell magnetic nano-material |
| CN105056965A (en) * | 2015-07-20 | 2015-11-18 | 长安大学 | Biological carbon sphere supported FeMoO4 Fenton catalyst, preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| N.SHARMA，ET AL.: ""Carbon-coated nanophase CaMoO4 as anode material for Li ion batteries"", 《CHEMISTRY MATERIAL》 * |
| QINGCHUN CHEN ET AL.: ""Fabrication of carbon microspheres@PbMoO4 core-shell hybrid structures and its visible light-induced photocatalytic activity"", 《CATALYSIS COMMUNICATIONS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824086A (en) * | 2017-03-20 | 2017-06-13 | 东华理工大学 | A kind of carbosphere Quito point loads the preparation method of heterogeneous structure material |
| CN112891532A (en) * | 2021-01-27 | 2021-06-04 | 深圳技术大学 | Nano photo-thermal conversion material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105016389B (en) | 2016-10-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhou et al. | Solar-to-hydrogen efficiency of more than 9% in photocatalytic water splitting | |
| Wang et al. | High-energy ball-milling constructing P-doped g-C3N4/MoP heterojunction with MoN bond bridged interface and Schottky barrier for enhanced photocatalytic H2 evolution | |
| Long et al. | Bamboo shoots shaped FeVO4 passivated ZnO nanorods photoanode for improved charge separation/transfer process towards efficient solar water splitting | |
| Li et al. | Direct electrodeposition of ZnO nanotube arrays in anodic alumina membranes | |
| Dubale et al. | Heterostructured Cu 2 O/CuO decorated with nickel as a highly efficient photocathode for photoelectrochemical water reduction | |
| Xing et al. | On the engineering part of solar hydrogen production from water splitting: photoreactor design | |
| Lin et al. | Hematite-based solar water splitting: challenges and opportunities | |
| CN106521547B (en) | A kind of TiO2/RGO/C3N4The Preparation method and use of combination electrode | |
| Tolod et al. | Visible light-driven catalysts for water oxidation: towards solar fuel biorefineries | |
| Bi et al. | Charge carrier dynamics investigation of Cu 2 S–In 2 S 3 heterostructures for the conversion of dinitrogen to ammonia via photo-electrocatalytic reduction | |
| Sajjadizadeh et al. | Engineering of a high-efficiency water splitting photoanode by synergistic effects of doping, compositing, and coupling on TiO2 nanoparticles | |
| Hamdani et al. | Cu2O nanowires based pn homojunction photocathode for improved current density and hydrogen generation through solar-water splitting | |
| CN104961159B (en) | A kind of nanometer tungsten oxide and one step vapour phase reduction preparation method and application | |
| Yuan et al. | Coke and sintering resistant nickel atomically doped with ceria nanosheets for highly efficient solar driven hydrogen production from bioethanol | |
| Yuan et al. | Photoelectrochemical reduction of carbon dioxide to methanol at CuS/CuO/CuInS2 thin film photocathodes | |
| Wannapop et al. | Enhanced visible light absorption of TiO2 nanorod photoanode by NiTiO3 decoration for high-performance photoelectrochemical cells | |
| Shi et al. | Defect engineering for tuning the photoresponse of ceria-based solid oxide photoelectrochemical cells | |
| Liao et al. | Open-top TiO 2 nanotube arrays with enhanced photovoltaic and photochemical performances via a micromechanical cleavage approach | |
| Liu et al. | Grey hematite photoanodes decrease the onset potential in photoelectrochemical water oxidation | |
| CN105016389B (en) | A kind of lead molybdate nanocrystal of carbon shell cladding and preparation method thereof | |
| CN108892170A (en) | A kind of " two phase process " prepares the BiVO of morphology controllable4Nanocrystalline method | |
| Wang et al. | Construction of a novel direct Z-scheme heterostructure consisting of ReS2 nanoflowers and In2S3 nanohoneycombs for improving photoelectrochemical performance | |
| Jin et al. | TiO 2 spatially confined growth of Sb 2 (S, Se) 3@ TiO 2 NT heterojunction photoanodes and their photoelectrochemical properties | |
| Zhao et al. | Preparation and photoelectric properties of praseodymium-doped cuprous oxide thin films | |
| CN102718491A (en) | Nanotube / powder blending phase metal oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161019 Termination date: 20200714 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |